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Spectroscopic Characterization of Wilkinson's Catalyst Using X-ray Photoelectron Spectroscopy (ESCA)

Volume 36, Number 3 (June 1982) Page 290-296

Carvalho, Manuel; Wieserman, Larry F.; Hercules, David M.


Wilkinson's catalyst, RhCl(PPh3)3 is a well known and widely used homogeneous hydrogenation catalyst. This catalyst was analyzed by ESCA which revealed that two rhodium species [Rh(I) and Rh(III)] were present, both for commercial preparations and for catalysts prepared in this laboratory. The ratio of Rh(I) to Rh(III) was 3:2 regardless of the source. A different method of synthesizing RhCl(PPh3)3 Wag used and produced a compound having only Rh(I) species. Additional analytical techniques such as elemental analysis, FT-IR, liquid chromatography, and 31P NMR were used to determine the origin of the higher binding energy peaks when Wilkinson's procedure was used to prepare RhCl(PPh3)3. Hydrogenation of cyclohexene was also performed to determine the effect of the higher binding energy species on catalytic activity.